CH87384A - Process for the manufacture of nitroguanidine. - Google Patents
Process for the manufacture of nitroguanidine.Info
- Publication number
- CH87384A CH87384A CH87384DA CH87384A CH 87384 A CH87384 A CH 87384A CH 87384D A CH87384D A CH 87384DA CH 87384 A CH87384 A CH 87384A
- Authority
- CH
- Switzerland
- Prior art keywords
- nitroguanidine
- manufacture
- sulfuric acid
- guanidine salt
- dicyandiamide
- Prior art date
Links
- IDCPFAYURAQKDZ-UHFFFAOYSA-N 1-nitroguanidine Chemical compound NC(=N)N[N+]([O-])=O IDCPFAYURAQKDZ-UHFFFAOYSA-N 0.000 title claims description 8
- 238000000034 method Methods 0.000 title claims description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 150000002357 guanidines Chemical class 0.000 claims description 5
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Procédé de fabrication de la nitroguanidine. On sait actuellement passer de la dicyan- diamide à la dieyandiamidine, de celle-ci aux sels de guauidine et de ces derniers préalable ment séparés à la nitroguanidine.
Ce procédé de préparation de la nitro- guanidine est pénible et coûteux.
Le procédé qui fait l'objet de la présente demande permet au contraire d'obtenir très rapidement la nitroguanidine dans un état de grande pureté, et avec d'excellents rende ments.
Suivant ce procédé, après transformation de la dicyandiamide en sel de guanidine par chauffage avec l'acide sulfurique, on trans forme ce dernier directement en nitroguani- dine dans la liqueur sulfurique même où il se trouve, sans séparation préalable, en ajoutant un mélange sulfo-nitrique à la solution sul furique du sel de guanidine.
<I>Exemple</I> On chauffe environ une heure au bain marie 84 grammes de dicyandiamide avec 336 grammes d'acide sulfurique à 61 /o d'HISOI'. On porte ensuite au bain d'huile à 135 - 140 ;
quand la transformation en sel de guanidine est totale (ce que l'on re- connait par un essai avec le réactif soude sulfate (le cuivre), ou laisse refroidir, et on ajoute à la niasse, .'t, une température inférieure à :
.'0 ", le mélange sulfonitrique suivant Acide Sulfurique F6 .92 "l" H-SOI . . . . 90(r Acide nitrique i1 40 Baumé . . . . 90" Tout se dissout. On coule alors la solu tion en la filtrant sur amiante dans l.,220" d'eau.
Après refroidissement, on filtre le tout; on obtient ainsi <B>87</B> grammes de nitro- guanidine, c'est-it-dire 84 0,'o environ du rende ment théorique.
Process for the manufacture of nitroguanidine. It is currently known to switch from dicyandiamide to dieyandiamidine, from the latter to guauidine salts and the latter previously separated to nitroguanidine.
This process for the preparation of nitroguanidine is laborious and expensive.
The process which is the subject of the present application, on the contrary, makes it possible to obtain nitroguanidine very quickly in a state of high purity, and with excellent yields.
According to this process, after conversion of the dicyandiamide into the guanidine salt by heating with sulfuric acid, the latter is transformed directly into nitroguanidine in the sulfuric liquor itself in which it is found, without prior separation, by adding a sulfo mixture. -nitric to the sulphuric solution of the guanidine salt.
<I> Example </I> 84 grams of dicyandiamide are heated for about an hour in a water bath with 336 grams of sulfuric acid at 61% HISOI '. It is then brought to an oil bath at 135-140;
when the conversion into the guanidine salt is complete (which is recognized by a test with the sodium sulphate reagent (copper), or left to cool, and we add to the mass, .'t, a temperature below :
.'0 ", the sulphonitric mixture according to Sulfuric Acid F6 .92" l "H-SOI... 90 (r Nitric acid i1 40 Baumé... 90" Everything dissolves. The solution is then poured into the mixture. filtering through asbestos in l. 220 "of water.
After cooling, the whole is filtered; this gives <B> 87 </B> grams of nitro-guanidine, ie about 84.0% of the theoretical yield.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR87384X | 1917-09-26 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CH87384A true CH87384A (en) | 1920-12-01 |
Family
ID=8763265
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CH87384D CH87384A (en) | 1917-09-26 | 1919-12-30 | Process for the manufacture of nitroguanidine. |
Country Status (1)
| Country | Link |
|---|---|
| CH (1) | CH87384A (en) |
-
1919
- 1919-12-30 CH CH87384D patent/CH87384A/en unknown
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